IJSR - INTERNATIONAL JOURNAL OF SCIENTIFIC RESEARCH 419 Volume : 5 | Issue : 10 | October 2016 • ISSN No 2277 - 8179 | IF : 3.508 | IC Value : 69.48 Original Research Paper Chemistry Sandip K. Jagadale S. B. Patil College of Engineering, Indapur, Pune 413106 Popatrao N. Bhosale Materials Research Laboratory, Department of Chemistry, Shivaji University, Kolhapur- 416004, Raghunath K. Mane Smt.K.R.P. Kanya Mahavidyalaya, Uran-Islampur, 415409 Tal.Walwa, Sangli, Route KEYWORDS : Nanocrystalline Thin Films, APT, XRD, SEM, XPS. ABSTRACT In the present investigation, we have synthesized nanocrystalline cadmium sulphoselenide Cd(SSe) thin ilms on ultrasonically cleaned bare and FTO coated glass substrate using facile, cost efective arrested precipitation technique (APT) at diferent time intervals (1h,1.5h, 2h and 2.5h). The absorption spectrum shows a strong absorption in the 300-1100 nm wavelength range with band gap variation in the range of 2.05 eV to 1.87 eV. The X-ray difraction (XRD) paterns shows nanocrystalline nature with crystallite size 58 nm to 76 nm and exhibits pure hexagonal crystal structure. The scanning electron microscopy (SEM) demonstrates for- mation of well adherent, pinhole free thin ilms with mixed nanosphere nanopetal like morphology. Energy dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) showed that the composition of Cd(SSe) thin ilms is good agreement with stoichiometry. Finally these prepared thin ilms tested for photoelectrochemical (PEC) performance in sulphide / polysulphide electrolyte and results are promising. INTRODUCTION The demand for the energy of the world is ever growing due to modern civilization and industrialization. To meet this demand of energy the conventional energy sources such as fossil fuels, natural oil, coal, etc. are mostly used which causes fast depletion of these reservoirs and also their combustion causes environmental pollution due to release of gases such as CO 2 and SO 2 . Solar energy is the clean, inexpensive and more eicient renewable energy op- tion for future energy demand. The photovoltaic solar cells convert sunlight directly into electricity and often used in many optoelectronic devices such as calculators and watches, etc. In last few decades, thin ilm based solar cells (TFSC) [1] have been commercialized due to their low cost of fabrication, high throughput processing techniques and ease of junction formation with a redox electrolyte to con- vert solar energy into electricity [2]. A variety of physical and chemical techniques have been employed for the synthesis of ternary Cd(SSe) thin ilms [3- 6]. In the present investigation, APT was used for synthesis of nanocrystalline Cd(SSe) thin ilms at diferent deposition time. Intention of present research work is to deposit na- nocrystalline Cd(SSe) thin ilms at diferent deposition time and also to study the inluence of deposition time on op- tostructural properties and its application in photoelectro- chemical solar cell. Experimental details All chemicals used in this work were analytical reagent (AR) grade and used without further puriication. Cadmium sulfate hy- drate (CdSO 4 .3H 2 O) (99 % Mereck), thiourea (NH 2 -CS-NH 2 ) (99 % Mereck), and Sodium selenosulite (Na 2 SeSO 3 ) were used as precursor for Cd 2+ , S 2- and Se 2- ions respectively. Sodium se- lenosulite (Na 2 SeSO 3 ) was prepared by reluxing selenium metal powder (99.5 % Lobachemie) and sodium sulite (Na 2 SO 3 ) (99 % Lobachemie) at 90 o C for 9 hrs. The excess concentration of Na 2 SO 3 over selenium prevents the oxidation of selenide and its reprecipitation as selenium. The pH of reaction bath was main- tained by ammonia (NH 3 ) (25 %, Thomas Baker) and triethanola- mine (TEA) used as complexing agent. For measuring the PEC performance, we have used a sulide/polysulide redox electrolyte prepared by crushing sodium sulide (Na 2 S) (55-58 % Thomas Baker), sodium hydroxide pellets (NaOH) (99 %, S-D Fine Chem.) and sulfur powder (99 %, S-D Fine Chem.) together and inally diluted to 50ml volume by double distilled water. Well cleaned commercial glass slides were used as substrate for thin ilm deposition. Synthesis of thin ilms Preparative parameters such as precursor concentration, com- plexing agent, pH, bath temperature and deposition time were optimized initially and the deposition time was varied from 1.0 to 1.5, 2.0, and 2.5 h. In a typical synthesis, an appropriate vol- ume of 0.05 M [Cd-TEA] solution was taken in a 100ml beak- er. The pH of the mixture was adjusted to 11 by dropwise ad- dition of ammonia followed by addition of adequate volume of 0.1 M Na 2 SeSO 3 and 0.1 M (NH 2 ) 2 C=S solution to the reaction mixture with constant stirring and then the reaction mixture was stirred for 2 min to get a homogeneous colorless solution. Pre- viously cleaned glass and luorine-doped tin oxide (FTO) coated glass substrates were mounted vertically on substrate holder with a constant rotation of 45±5 rpm. At this stage nucleation centers are formed on substrate surface at 55 ± 2 o C followed by ion by ion condensation mechanism which results in formation of well adherent, uniform and pinhole free thin ilm on substrate surface [7]. After desired deposition time, the substrates were withdrawn from the reaction bath, suficiently rinsed with double-distilled water and dried at room temperature and correspondingly desig- nated as CSS1, CSS2, CSS3 and CSS4. It could be seen that, for the terminal growth of the ilms, the ilm thickness remains con- stant after 2.5 h. So, we have studied the inluence of deposition time for up to 2.5 h. Characterization of the thin ilms The thickness of as deposited thin ilms was measured by us- ing surface proiler (AMBIOS XP-1). UV-Vis-NIR absorbance spectra were measured using a model Shimadzu UV 1800 in the wavelength range 300 nm to 1100 nm. The crystal structure of the thin ilms were analyzed by X-ray powder diffraction (XRD) with Rigaku, D/MAX Ultima III XRD spectrometer (Japan) us- ing Cu-Kα radiation (λ = 1.5418 Å) in 20 o to 80 o 2θ range. The surface morphology elemental composition of Cd(SSe) thin ilms were assessed by scanning electron microscope (SEM) equipped with energy dispersive X-ray spectroscopy (EDS) analyzer (JE- OL-JSM- 6360A). Elemental composition of Cd(SSe) thin ilms can obtained by energy dispersive X-ray spectroscopy (EDS) ana- lyzer (JEOL-JSM- 6360A) and X-ray photoelectron spectroscopy. The PEC performance were measured in dark conditions and un- der irradiation of light using a 500 W tungsten ilament lamp (in- tensity 30 mW/cm 2 ) at an electrochemical workstation (AUTO- LAB PGSTAT 100 potentiostat) with two electrode coniguration, Efect of Deposition Time on Optostructural and Photoelectrochemical Properties of Cd(SSe) Thin Films Deposited By Facile